CN106632931A - Preparation method of organic silicone-modified phenolic resin friction powder - Google Patents
Preparation method of organic silicone-modified phenolic resin friction powder Download PDFInfo
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- CN106632931A CN106632931A CN201611007182.0A CN201611007182A CN106632931A CN 106632931 A CN106632931 A CN 106632931A CN 201611007182 A CN201611007182 A CN 201611007182A CN 106632931 A CN106632931 A CN 106632931A
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- phenolic resin
- linseed oil
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical class [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 235000021388 linseed oil Nutrition 0.000 claims abstract description 41
- 239000000944 linseed oil Substances 0.000 claims abstract description 41
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 39
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 25
- 239000005011 phenolic resin Substances 0.000 claims abstract description 25
- JWAZRIHNYRIHIV-UHFFFAOYSA-N 2-naphthol Chemical compound C1=CC=CC2=CC(O)=CC=C21 JWAZRIHNYRIHIV-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 16
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229950011260 betanaphthol Drugs 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010792 warming Methods 0.000 claims description 27
- 238000006243 chemical reaction Methods 0.000 claims description 24
- 230000000694 effects Effects 0.000 claims description 18
- 239000012467 final product Substances 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 6
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 6
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 6
- 239000011425 bamboo Substances 0.000 claims description 6
- 239000004917 carbon fiber Substances 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 6
- 239000011790 ferrous sulphate Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 239000004312 hexamethylene tetramine Substances 0.000 abstract 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 abstract 1
- 229960004011 methenamine Drugs 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 244000226021 Anacardium occidentale Species 0.000 description 12
- 235000020226 cashew nut Nutrition 0.000 description 12
- 239000007788 liquid Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 238000006116 polymerization reaction Methods 0.000 description 6
- 241001330002 Bambuseae Species 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 238000001879 gelation Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 230000004580 weight loss Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000746 allylic group Chemical group 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- JUHDUIDUEUEQND-UHFFFAOYSA-N methylium Chemical compound [CH3+] JUHDUIDUEUEQND-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 125000002769 thiazolinyl group Chemical group 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/30—Chemically modified polycondensates by unsaturated compounds, e.g. terpenes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention relates to a preparation method of organic silicone-modified phenolic resin friction powder. The method comprises the steps of putting beta-naphthol, formaldehyde and ammonia water into a reactor, stirring while heating until the temperature is 100-120 DEG C, and reacting for 40-60min; adding butanol for dehydrating, and rapidly cooling when heating up to 150 DEG C, so as to obtain phenolic resin; adding dimethyldichlorosilane, modified linseed oil and maleic anhydride into the reactor, stirring while heating until the temperature is 220-240 DEG C, and reacting for 80-100min; slowly adding the phenolic resin, heating up to 240-250 DEG C, and reacting for 10-80min; adding butanol when naturally cooling to 110-120 DEG C, reacting for 10-40min, adding hexamethylene tetramine when the temperature is 50-55 DEG C, fully mixing and then heating up to 150-200 DEG C, reacting for 6-8h, grinding and screening. Probably because of the higher crosslinking density of the organic silicone-modified phenolic resin, the organic silicone-modified phenolic resin friction powder is higher in friction resisting ability.
Description
Technical field
The present invention relates to a kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder.
Background technology
Friction-type mix, is widely used as the additive of various abrasiveses, can play stable coefficient of friction, reduce noise,
The effect of abrasion is reduced, can be used for the brake shoe of the motor vehicles such as automobile train and the clutch surface of a gearing
Piece.Prior art application it is more be cashew nut shell oil Frication powder, with the rising of temperature, cashew nut shell oil composition therein makes friction
Material is relatively stable with the contact of antithesis, especially compared with other organic materials, there is more preferable stability.
The patent application of Application No. CN201310328255.6 discloses a kind of Cashew nut shell liquid friction powder and its preparation side
Method, with sufficient raw, makes full use of reproducible cashew nut shell liquid, with dithyl sulfate as catalyst, by cashew nut shell
More active double bond forms allylic carbon cation and initiated polymerization in anacardol unsaturation thiazolinyl in liquid, and what is obtained is poly-
Cashew nut shell liquid compound and furfural are closed, in presence of an acid catalyst, filler is added, gelation is carried out, is carried out again after gelation thick
It is broken, curing reaction is then carried out, cured product discharging simultaneously Jing after levigate, can obtain Cashew nut shell liquid friction powder, specifically comprising following step
Suddenly：1). with dithyl sulfate as catalyst, at 190 DEG C～210 DEG C, 3～5h of back flow reaction completes cashew nut shell to cashew nut shell liquid
The polymerization of liquid, generates main polymerization cashew nut shell liquid compound, according to the iodine number and viscosity that determine polymerization cashew nut shell liquid compound
Judge extent of polymerization；2). the polymerization cashew nut shell liquid compound of generation, in presence of an acid catalyst, furfural is added, carry out gelation
Reaction, carries out again coarse crushing after material gelation, then in 180～200 DEG C of 15～20h of curing reaction, cured product discharges and Jing
Frication powder is obtained final product after levigate.
The content of the invention
The purpose of the present invention is：A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder is provided, it is heat-resist and
Crocking resistance is strong.
Technical scheme is：
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, betanaphthol, formaldehyde and ammoniacal liquor are put in reactor, are heated while stir, and to 100～120 DEG C 40 are reacted
～60min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, modified linseed oil, maleic anhydride are added in reactor, are heated to while stirring
220～240 DEG C, 80～100min is reacted, be then slowly added into the phenolic resin of the 1st step, be warming up to 240～250 DEG C of reactions 10
～80min；
3rd step, is naturally cooling to add butanol when 110～120 DEG C, reacts 10～40min, and during to 50～55 DEG C six methylenes are added
Urotropine, is warming up to 150～200 DEG C of 6～8h of reaction after being sufficiently mixed, pulverize and sieve, and obtains final product.
In the 1st described step, in parts by mass, 3～20 parts of 2～4 parts of betanaphthol, 1～5 part of formaldehyde and ammoniacal liquor.Formaldehyde contains
Amount is too small to be easily caused resin viscosity reduction, it is not easy to solidify.
In the 1st described step, betanaphthol, the mass ratio of formaldehyde are 2：1.
In the 2nd described step, in parts by mass, 10～12 parts of dimethyldichlorosilane, be modified 30～40 parts of linseed oil, suitable
12～15 parts of anhydride maleique, 100～150 parts of phenolic resin.
In the 2nd described step, when the consumption of maleic anhydride is the 13.6% of phenolic resin consumption, heat resistance is best.
In the 2nd described step, the preparation method of modified linseed oil is：First linseed oil is heated to into 50-60 DEG C, then to it
2-3% ferrous sulfate, 5～10% carbon fibers, 2～7% bamboo fibres of middle addition flax oil quality；It is uniformly mixed placement 1～3
Hour, the sodium humate powder of linseed oil 10～20% is then added, uniform stirring 5～6 under conditions of being warming up to 70～80 DEG C
Hour, room temperature is naturally cooled to, solution ph is adjusted to 2～3；Again with deionized water in mass ratio 1:7 mixing, stirring 30～40
Minute, centrifugation obtains filtrate, and the above is in parts by mass.
Beneficial effect
The present invention has preferable heat resistance, at 200 DEG C it is weightless seldom, the thermal weight loss rate at 400 DEG C is also only 12% left
It is right.The rub resistance ability of the present invention is stronger, and the crosslink density that this is possibly due to Effect of Organosilicon-modified Phenol-formaldehyde Resin of the present invention is higher.
Specific embodiment
Embodiment 1
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, in parts by mass, by 2 parts of betanaphthol, 10 parts of input reactors of 1 part of formaldehyde and ammoniacal liquor, heats while stirring
Mix, to 110 DEG C of reaction 50min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, modified linseed oil, maleic anhydride are added in reactor, are heated to while stirring
230 DEG C, 90min is reacted, be then slowly added into the phenolic resin of the 1st step, be warming up to 245 DEG C of reaction 50min；In parts by mass,
11 parts of dimethyldichlorosilane, be modified 35 parts of linseed oil, 13.6 parts of maleic anhydride, 100 parts of phenolic resin；
3rd step, is naturally cooling to add butanol when 115 DEG C, reacts 30min, and during to 53 DEG C hexa is added, fully mixed
180 DEG C of reaction 7h are warming up to after conjunction, are pulverized and sieved, obtained final product.
The preparation method of the modified linseed oil is：First linseed oil is heated to into 55 DEG C, is then added thereto to linseed oil
2.5% ferrous sulfate of quality, 8% carbon fiber, 5% bamboo fibre；Placement 2 hours is uniformly mixed, linseed oil is then added
15% sodium humate powder, uniform stirring 5.6 hours under conditions of being warming up to 75 DEG C naturally cool to room temperature, adjust pH value of solution
It is worth to 2.3；Again with deionized water in mass ratio 1:7 mixing, stirring 35 minutes, centrifugation obtains filtrate, and the above presses quality
Part meter.
Embodiment 2
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, in parts by mass, by 3 parts of betanaphthol, 3 parts of input reactors of 4 parts of formaldehyde and ammoniacal liquor, heats while stirring
Mix, to 100 DEG C of reaction 40min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, modified linseed oil, maleic anhydride are added in reactor, are heated to while stirring
220 DEG C, 80min is reacted, be then slowly added into the phenolic resin of the 1st step, be warming up to 240 DEG C of reaction 10min；In parts by mass,
10 parts of dimethyldichlorosilane, be modified 30 parts of linseed oil, 12 parts of maleic anhydride, 120 parts of phenolic resin；
3rd step, is naturally cooling to add butanol when 110 DEG C, reacts 10min, and during to 50 DEG C hexa is added, fully mixed
150 DEG C of reaction 6h are warming up to after conjunction, are pulverized and sieved, obtained final product.
The preparation method of the modified linseed oil is：First linseed oil is heated to into 50 DEG C, is then added thereto to linseed oil
2% ferrous sulfate of quality, 5% carbon fiber, 2% bamboo fibre；Placement 1 hour is uniformly mixed, linseed oil 10% is then added
Sodium humate powder, uniform stirring 5 hours under conditions of being warming up to 70 DEG C naturally cool to room temperature, adjust solution ph to
2；Again with deionized water in mass ratio 1:7 mixing, stirring 30 minutes, centrifugation obtains filtrate, and the above is in parts by mass.
Embodiment 3
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, in parts by mass, by 4 parts of betanaphthol, 20 parts of input reactors of 5 parts of formaldehyde and ammoniacal liquor, heats while stirring
Mix, to 120 DEG C of reaction 60min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, modified linseed oil, maleic anhydride are added in reactor, are heated to while stirring
240 DEG C, 100min is reacted, be then slowly added into the phenolic resin of the 1st step, be warming up to 250 DEG C of reaction 80min；In parts by mass,
12 parts of dimethyldichlorosilane, be modified 40 parts of linseed oil, 15 parts of maleic anhydride, 150 parts of phenolic resin；
3rd step, is naturally cooling to add butanol when 120 DEG C, reacts 40min, and during to 55 DEG C hexa is added, fully mixed
200 DEG C of reaction 8h are warming up to after conjunction, are pulverized and sieved, obtained final product.
The preparation method of the modified linseed oil is：First linseed oil is heated to into 60 DEG C, is then added thereto to linseed oil
3% ferrous sulfate of quality, 10% carbon fiber, 7% bamboo fibre；Placement 3 hours is uniformly mixed, linseed oil 20% is then added
Sodium humate powder, uniform stirring 6 hours under conditions of being warming up to 80 DEG C naturally cool to room temperature, adjust solution ph to
3；Again with deionized water in mass ratio 1:7 mixing, stirring 40 minutes, centrifugation obtains filtrate, and the above is in parts by mass.
Reference examples 1
It is with the difference of embodiment 3：Modified linseed oil is replaced using common linseed oil.
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, in parts by mass, by 4 parts of betanaphthol, 20 parts of input reactors of 5 parts of formaldehyde and ammoniacal liquor, heats while stirring
Mix, to 120 DEG C of reaction 60min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, linseed oil, maleic anhydride are added in reactor, and 240 are heated to while stirring
DEG C, 100min is reacted, the phenolic resin of the 1st step is then slowly added into, it is warming up to 250 DEG C of reaction 80min；In parts by mass, two
12 parts of dimethyl dichlorosilane (DMCS), 40 parts of linseed oil, 15 parts of maleic anhydride, 150 parts of phenolic resin；
3rd step, is naturally cooling to add butanol when 120 DEG C, reacts 40min, and during to 55 DEG C hexa is added, fully mixed
200 DEG C of reaction 8h are warming up to after conjunction, are pulverized and sieved, obtained final product.
Reference examples 2
It is with the difference of embodiment 3：Dimethyldichlorosilane is not added with 2nd step.
A kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, comprises the steps：
1st step, in parts by mass, by 4 parts of betanaphthol, 20 parts of input reactors of 5 parts of formaldehyde and ammoniacal liquor, heats while stirring
Mix, to 120 DEG C of reaction 60min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, modified linseed oil, maleic anhydride are added in reactor, 240 DEG C are heated to while stirring, reaction
100min, is then slowly added into the phenolic resin of the 1st step, is warming up to 250 DEG C of reaction 80min；In parts by mass, be modified linseed oil
40 parts, 15 parts of maleic anhydride, 150 parts of phenolic resin；
3rd step, is naturally cooling to add butanol when 120 DEG C, reacts 40min, and during to 55 DEG C hexa is added, fully mixed
200 DEG C of reaction 8h are warming up to after conjunction, are pulverized and sieved, obtained final product.
The preparation method of the modified linseed oil is：First linseed oil is heated to into 60 DEG C, is then added thereto to linseed oil
3% ferrous sulfate of quality, 10% carbon fiber, 7% bamboo fibre；Placement 3 hours is uniformly mixed, linseed oil 20% is then added
Sodium humate powder, uniform stirring 6 hours under conditions of being warming up to 80 DEG C naturally cool to room temperature, adjust solution ph to
3；Again with deionized water in mass ratio 1:7 mixing, stirring 40 minutes, centrifugation obtains filtrate, and the above is in parts by mass.
The product for obtaining made above is tested, it is as a result as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Reference examples 1 | Reference examples 2 | |
| Thermal weight loss rate % when 200 DEG C | 5 | 4 | 5 | 13 | 10 |
| Thermal weight loss rate % when 400 DEG C | 12 | 11 | 11 | 38 | 29 |
| Coefficient of friction when 200 DEG C | 0.7 | 0.7 | 0.7 | 0.4 | 0.3 |
| Coefficient of friction when 400 DEG C | 0.6 | 0.5 | 0.6 | 0.2 | 0.1 |
As can be seen from the above table, compared with reference examples 1, the present invention has preferable heat resistance, weightless little at 200 DEG C,
Thermal weight loss rate at 400 DEG C also only has 12% or so.Compared with reference examples 2, the rub resistance ability of the present invention is stronger, and this may
It is because that the crosslink density of Effect of Organosilicon-modified Phenol-formaldehyde Resin of the present invention is higher.
Claims (6)
1. a kind of preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder, it is characterised in that comprise the steps：
1st step, betanaphthol, formaldehyde and ammoniacal liquor are put in reactor, are heated while stir, and to 100～120 DEG C 40 are reacted
～60min；Butanol dehydration is added, when being warming up to 150 DEG C, rapid cooling obtains phenolic resin, standby；
2nd step, dimethyldichlorosilane, modified linseed oil, maleic anhydride are added in reactor, are heated to while stirring
220～240 DEG C, 80～100min is reacted, be then slowly added into the phenolic resin of the 1st step, be warming up to 240～250 DEG C of reactions 10
～80min；
3rd step, is naturally cooling to add butanol when 110～120 DEG C, reacts 10～40min, and during to 50～55 DEG C six methylenes are added
Urotropine, is warming up to 150～200 DEG C of 6～8h of reaction after being sufficiently mixed, pulverize and sieve, and obtains final product.
2. the preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder according to claim 1, it is characterised in that described
In 1st step, in parts by mass, 3～20 parts of 2～4 parts of betanaphthol, 1～5 part of formaldehyde and ammoniacal liquor.
3. the preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder according to claim 2, it is characterised in that described
In 1st step, betanaphthol, the mass ratio of formaldehyde are 2：1.
4. the preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder according to claim 1, it is characterised in that described
In 2nd step, in parts by mass, 10～12 parts of dimethyldichlorosilane, be modified 30～40 parts of linseed oil, maleic anhydride 12～
15 parts, 100～150 parts of phenolic resin.
5. the preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder according to claim 4, it is characterised in that described
In 2nd step, when the consumption of maleic anhydride is the 13.6% of phenolic resin consumption, heat resistance is best.
6. the preparation method of Effect of Organosilicon-modified Phenol-formaldehyde Resin Frication powder according to claim 1, it is characterised in that described
In 2nd step, the preparation method of modified linseed oil is：First linseed oil is heated to into 50-60 DEG C, is then added thereto to flax oil
The 2-3% ferrous sulfate of amount, 5～10% carbon fibers, 2～7% bamboo fibres；It is uniformly mixed placement 1～3 hour, then adds
The sodium humate powder of linseed oil 10～20%, uniform stirring 5～6 hours, naturally cool under conditions of being warming up to 70～80 DEG C
Room temperature, adjusts solution ph to 2～3；Again with deionized water in mass ratio 1:7 mixing, stirring 30～40 minutes, centrifugation is obtained
Filtrate, the above is in parts by mass.
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| WO2018098923A1 (en) * | 2016-12-02 | 2018-06-07 | 广东生益科技股份有限公司 | Styryl siloxy phenolic resin, preparation method therefor and application thereof |
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| CN1072188A (en) * | 1991-11-05 | 1993-05-19 | 成都科技大学 | The manufacturing of tung oil modified linear phenol-aldehyde resin and application |
| CN1752122A (en) * | 2005-09-29 | 2006-03-29 | 江苏大学 | Linseed oil modified phenol formaldehyde resin for friction material and its preparation method |
| CN101798436A (en) * | 2010-03-12 | 2010-08-11 | 江苏大学 | Boron and linseed oil double-modification phenolic resin-based friction resistance composite material and preparation method thereof |
| CN103068948A (en) * | 2010-08-26 | 2013-04-24 | 昭和电工株式会社 | Wet friction material |
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| CN1072188A (en) * | 1991-11-05 | 1993-05-19 | 成都科技大学 | The manufacturing of tung oil modified linear phenol-aldehyde resin and application |
| CN1752122A (en) * | 2005-09-29 | 2006-03-29 | 江苏大学 | Linseed oil modified phenol formaldehyde resin for friction material and its preparation method |
| CN101798436A (en) * | 2010-03-12 | 2010-08-11 | 江苏大学 | Boron and linseed oil double-modification phenolic resin-based friction resistance composite material and preparation method thereof |
| CN103068948A (en) * | 2010-08-26 | 2013-04-24 | 昭和电工株式会社 | Wet friction material |
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